Experiment 5

Percent Water in a Hydrated Salt

A gravimetric analysis is used to determine the percent by mass of water in a
INTRODUCTION hydrated salt. This is the first experiment requiring quantitative data collection and
analysis. The Techniques section of the manual should be referred to often.
While the experiment refers to crucible and crucible lid as the apparatus of choice, a 150-mm
(6”) test tube may be substituted with similar results. The thermal decomposition
temperatures of the hydrated salts do not mandate the use of a crucible.
Work Arrangement: Individuals. Three trials to determine the mass of water in the
hydrated salt are recommended.
Time Requirement: 3 hours (including calculations)
1. Follow the Instruction Routine outlined in “To the Laboratory Instructor”.
LECTURE 2. Provide an overview of the Experimental Procedure.
OUTLINE 3. Impress upon students the quantitative nature of this analysis. Students should
only use crucible tongs when handling the crucible and lid once the crucible and
lid have been fired (see Figure 5.2) for two reasons…so that oily fingers do not
affect the mass measurements and so that fingers are not burned!
4. Demonstration. Demonstrate the technique for handling a crucible and lid with
crucible tongs (or test tube with a test tube holder).
5. A sample calculation for showing the percent water in a hydrated salt may be
helpful (for example, Prelaboratory Assignment, Q#5).
6. Three analyses require you and the students to be well prepared. Time spent in
the balance area should not be wasted. If the equipment is available, it is
advisable to have three (3) crucible/lid or test tube setups.
7. Review with the students, or impress upon the students, the importance of
technique when heating substances in a crucible as discussed in Technique 15C.
The Next Step. Numerous analyses require heating samples to dryness to
investigate the composition of a sample. The manual provides a number of
suggestions…if coal samples are available, suggestion #3 is a very informative
analysis. Extra credit?
• Footnote 2. Carefully handle the 6 M HNO3. It is advisable to discourage
CAUTIONS students from cleaning their crucible in Part A with the nitric acid.
& DISPOSAL • Hot and cold crucibles look the same! Do not touch! Burned fingertips are
common to those students who are careless or do not wish to develop the
technique of handling the crucible and lid with crucible tongs.
• Do not place a hot crucible on the balance pan or on the benchtop.
• Anhydrous salts should be discarded in the “Waste Solids” container.
1. Part A.1. Have students closely inspect their crucible—hairline fissures are
TEACHING HINTS places along which crucibles ultimately break. Do not continue with the
experiment if a hairline fissure is observed. Have students check out a
replacement crucible.
2. Part A.1, footnote 2. To remove difficult stains and/or carbon deposits from
crucibles, add 2–3 mL of 6 M HNO3, transfer to a fume hood, and heat to
dryness. This procedure should be used with discretion. Only responsible
students with good laboratory technique should clean crucibles with nitric acid.
3. Part A.1. Only cool crucibles are to be placed on the balance pan. If available, the
crucible and lid should be allowed to cool in a desiccator.
4. Part A.2. Limit the amount of hydrated salt that is analyzed—the more salt that
is used, the longer is the time period for removing the hydrated water molecules.

22 Percent Water in a Hydrated Salt

5. Part A.2. Advise students to record the masses to the sensitivity of the balance,
i.e., the correct number of significant figures; see Data Analysis, A.
6. Part B.1. Heat the crucibles containing the sample slowly at first and then
gradually intensify the heat.
7. Part B.2. Do not overheat the salt; this avoids its decomposition.
8. Part B.2. Repeated mass measurements of the crucible after the water has been
removed should be within ± 0.010 g.
9. Part B.3. Results should agree to <3%.
6 M HNO3 2–5 mL
1 M HCl 2–3 mL CHEMICALS
REQUIRED
A 3-g sample of a hydrated salt is required per trial; for three trials a mass of
about 10 g is required per student. SUGGESTED
UNKNOWNS
SrCl2•6H2O (loses 5 H2O at 100°C, 6 H2O at 150°C)
Na2CO3•H2O (loses 1 H2O at 100°C)
ZnSO4•7H2O (loses 7 H2O at 280°C)
CaSO4•2H2O (loses 1 1/2 H2O at 128°C, 2 H2O at 163°C)
CuSO4•5H2O (loses 4 H2O at 110°C, 5 H2O at 150°C)
MgSO4•7H2O (loses 6 H2O at 150°C, 7 H2O at 200°C)
crucible tongs
crucible and lid 3 SPECIAL
clay triangle 1 EQUIPMENT
balances, ±0.001 g
fume hood
Bunsen burner
ring stand and iron support ring
desiccator or desicooler (optional)
“Waste Solids” container
“Waste Acids” container
1. Anhydrous calcium chloride CaCl2, being deliquescent, readily absorbs water
from the atmosphere to form CaCl2•2H2O. Stored in a dessicator it creates a dry PRELABORATORY
atmosphere in which to store chemicals. ASSIGNMENT
2. The crucible is fired to remove any existing stains or impurities that had
previously adhered to the crucible. The crucible is, in effect, “cleaned” by
heating it to a very high temperature.
1.803 g - 1.426 g
3. 1.803 g x 100 = 20.91% H2O
4. a. Contaminants from the fingers (e.g., fingerprints) or gloves can be
transferred to the crucible and lid to cause an error in mass measurements.
Using crucible tongs to handle the crucible eliminates this potential error.
b. When the crucible and lid are above room temperature, induced convection
currents about the pan of the balance can affect the mass reading of the
balance. The mass reading is likely to be too low as a result.

Experiment 5 23
 5.
Trial 1 Trial 2 Trial 3
Mass of fired crucible and lid 19.437 20.687 18.431
(g)
Mass of fired crucible, lid, and 21.626 25.111 22.167
hydrated salt (g)
Final mass of fired crucible, 21.441 24.702 21.762
lid, and anhydrous salt (g)
Calculations
1. Mass of hydrated salt (g) 2.189 4.424 3.736
2. Mass of anhydrous salt (g) 2.004 4.015 3.331
3. Mass of water lost (g) 0.185 0.409 0.405
4. Percent by mass of volatile
water in hydrated salt (%) 8.45 9.25 10.84
5. Average percent H2O in 9.51
hydrated salt (%H2O)
6. Standard deviation of 1.22 (1.06)2 + (0.26)2 + (1.33)2
%H2O
3 –1
7. Relative standard 1.22 x 100
deviation of %H2O in 12.8 9.51
hydrated salt (%RSD)
126.07 g H2O
6. a. 277.98 g FeSO4•7H2O x 100 = 45.352% H2O
45.352 g H2O
b. 3.38 g FeSO4•7H2O x 100 g FeSO •7H = 1.53 g H2O
4 2O

1. Too high. A larger than actual mass loss will occur if the crucible initially has
LABORATORY occluded moisture (lost in the heating process) and this additional mass will be
QUESTIONS calculated as water loss from the sample.
2. Too high. The fingerprints will calculate as a mass loss in the heating process and
will contribute to a water loss. This additional mass will be calculated as a mass
loss due to water from the sample.
3. Too high. The mass of oil from the fingers will be considered a part of the sample.
Since it will be an additional loss (along with the water) when the sample is
heated, the percent water will be calculated too high while the mass of the
mass of water
sample will remain unchanged…%H2O = mass of sample x 100.
4. Too low. The mass of the anhydrous salt will contribute to the total mass of the
mixture, but the anhydrous material will not lose water. With a higher than
actual mass of salt, the percent water of the “assumed” pure hydrated salt will be
too low.
*5. Too low. The oil from the lab bench would be considered a part of the hydrated
salt. In the heating process, the waters of hydration and the oil would be
volatilized, leaving the measured mass of the anhydrous salt as being too low.
6. Too high. The mass of the remaining anhydrous salt would be too low, resulting
in a calculated higher percent water in the sample.
7. Too high. The mass loss of the solid due to the spattering will be calculated as a
greater mass loss of water and thus a higher reported percent water in the
hydrated salt.
8. Too low. It is unlikely that all water will be driven off after the first heating,
leaving waters of hydration still bonded to the salt, resulting in a reported
percent water in the salt as being too low.

24 Percent Water in a Hydrated Salt

1. Write the formula of the heptahydrate salt of ferrous sulfate. LABORATORY
[Answer: FeSO4•7H2O]
2. How many grams of water are in 5.00 g of CuSO4•5H2O (molar mass = 249.7
QUIZ
g/mol)? [Answer: 1.80 g]
3. A hydrated salt is heated to determine the percent water in the salt.
a. If all of the hydrated water molecules are not removed, is the calculated
percent water in the salt reported too high or too low? Explain.
[Answer: % H2O is too low]
b. If the hydrated salt is overheated to the extent that the salt decomposes into a
volatile product, is the calculated percent water in the salt reported too high
or too low? Explain. [Answer: %H2O is reported too high]
4. In an experiment, the hydrated salt was heated according to the accepted
experimental procedure; however, the sample was allowed to cool without the
crucible being covered. Will the mass of water in the salt be reported too high or
too low? Explain.
[Answer: Too low. The anhydrous salt absorbs water from the atmosphere as the
sample cools.]
5. A 2.789-g sample of a hydrated sodium carbonate salt was heated in a crucible.
After heating, a reproducible mass of 2.384 g of anhydrous sodium carbonate
was obtained. What is the percent by mass of water in the hydrated sodium
carbonate salt? [Answer: 14.5% H2O]
6. What error in the data is likely to occur if the hydrated salt is heated too
strongly?
[Answer: The anhydrous salt itself may decompose and the percent water is reported
too high.]
7. If the hydrated water molecules are not completely removed from the salt during
the heating process, will the reported percent water in the salt be too high or too
low? Explain.
[Answer: Too low. The remaining partially hydrated solid will be considered
anhydrous salt, resulting in a smaller mass of water removed.]
8. Anhydrous CaCl2 removes water vapor from the air inside a container having an
airtight seal—this apparatus is called a desiccator. Discuss how the calcium
chloride removes the water vapor.
[Answer: CaCl2 adsorbs water vapor from the atmosphere into its crystalline
structure, forming a hydrated calcium chloride salt (CaCl2•2H2O).]

Experiment 5 25